CN103143392B - Method for preparing phenolic aldehyde amine (PAA)/polyvinyl acetate (PVA) nano-fiber felt containing Au dendrimer-stabilized nanoparticles (DSNPs) - Google Patents

Method for preparing phenolic aldehyde amine (PAA)/polyvinyl acetate (PVA) nano-fiber felt containing Au dendrimer-stabilized nanoparticles (DSNPs) Download PDF

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CN103143392B
CN103143392B CN201310067293.0A CN201310067293A CN103143392B CN 103143392 B CN103143392 B CN 103143392B CN 201310067293 A CN201310067293 A CN 201310067293A CN 103143392 B CN103143392 B CN 103143392B
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dsnps
paa
pva
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nanofiber mats
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CN103143392A (en
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史向阳
胡登脉
黄云鹏
刘辉
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Donghua University
National Dong Hwa University
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Abstract

The invention relates to a method for preparing a phenolic aldehyde amine (PAA)/polyvinyl acetate (PVA) nano-fiber felt containing Au dendrimer-stabilized nanoparticles (DSNPs). The method comprises the following steps of: preheating a polyamide-imide dendrimer aqueous solution, then adding a chloroauric acid solution, stirring to react for 2-3 hours, and cooling and drying so as to obtain the Au dendrimer-stabilized nanoparticles (DSNPs); preparing PAA/PVA polyelectrolyte spinning solution, wherein the weight ratio of PAA to PVA is 1:(1-2); electrostatically spinning so as to obtain the nano-fiber felt, and then crosslinking and performing water-stabilized treatment on the nano-fiber felt; and soaking the nano-fiber felt in water for 2-4 hours, then adding Au dendrimer-stabilized nanoparticles (DSNPs) aqueous solution, and shaking and vacuum drying so as to obtain a product. The method is simple, and the product is easy to prepare; and the Au nanoparticles which are combined with a fibrous membrane through a physical method have high catalytic efficiency and good reutilization performance as well as a wide application scope in the fields of catalysis, environmental modification and the like.

Description

A kind of preparation method of the PAA/PVA nanofiber mats containing Au DSNPs
Technical field
The invention belongs to the preparation field of composite nanometer fiber felt, particularly a kind of preparation method of the PAA/PVA nanofiber mats containing Au DSNPs.
Background technology
Metal nanoparticle is owing to having size and pattern dependence, thereby the metal nanoparticle of different size often shows the physicochemical properties of many uniquenesses, and this has evoked people to metal nano material keen interest.Wherein most important is exactly application study about nano material.In recent years, emerge in an endless stream at the bibliographical information of the field application studies such as optics, biology sensor, drug delivery, medical imaging, catalysis about metal nano material.Metal nano material is particularly rapid in catalytic field development.The various metals nano materials such as current gold, silver, copper, palladium obtain reasonable application at catalytic field.For example Esumi(Kazutaka Hayakawa, Tomokazu Yoshimura, Kunio Esumi.Preparation of gold-dendrimer nanocomposites by laser irradiation and their catalytic reduction of4-nitrophenol.Langmuir2003,19,5517-5521) etc. people has prepared the nm of gold composite of dendrimer parcel, and by this kind of composite for the reduction reaction of catalysis tetranitro-phenol, show fabulous catalytic effect.But this kind of composite is difficult to recycling and the shortcoming that is difficult for reclaiming is restricted its application.
Electrostatic spinning is a kind of simple and efficient nanofiber forming technique.The nanofiber of preparing by method of electrostatic spinning has the advantages such as specific area is large, porosity is high, draw ratio is large, mechanical property is good.These advantages of electrostatic spinning technique, make it all have a wide range of applications in fields such as reinforcing material, biomedicine, porous material, electrode material, catalyst carriers.In work before this seminar, prepare with in-situ synthesis Static Spinning polymine/polyacrylic acid nano fibrofelt (the Fang et al.J.Mater.Chem.2011 that contains gold nano grain, 21 (12), 4493-4501), and this catalytic performance containing gold nano fibrous composite is tested, obtain good result.
Nano composite material prepared by above-mentioned in-situ reducing method is except fiber surface has metal nanoparticle, and fibrous inside also has a large amount of nano particles.In order further to improve the catalytic activity containing gold nano fibrous composite, the assemble method of nano surface particle also obtains people's favor gradually.Retrieve domestic and international pertinent literature and not yet find that there is the report that gold nano grain stable dendrimer is assembled into fiber surface.We obtain nano-fiber composite material by gold nano grain stable second generation Polyamidoamine Dendrimers is assembled into fiber surface, overcome on the one hand the shortcoming of difficult recovery when the stable gold nano grain of dendrimer is used as catalyst, utilize on the other hand the advantage of the specific area that electrostatic spinning fiber felt is large, being assembled in fiber surface will improve the catalytic performance of nano particle greatly.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of the PAA/PVA nanofiber mats containing Au DSNPs, and that the method has is simple to operation, raw material easily reclaims, environmental pollution is little, be applicable to the advantages such as large-scale production.The gold nano grain of uploading by this preparation method is stablized, nothing is reunited, and is evenly distributed on fiber surface.
The preparation method of a kind of PAA/PVA nanofiber mats containing Au DSNPs of the present invention, comprising:
(1) by the preheating of the Polyamidoamine Dendrimers aqueous solution, then add chlorauric acid solution, stirring reaction 2-3h, cool drying, obtains the stable gold nano grain Au DSNPs of dendrimer; Wherein the mol ratio of gold and dendrimer is 3:1;
(2) the polyelectrolyte spinning solution of the polyacrylic acid PAA/ PVAC polyvinylalcohol that preparation weight ratio is 1:1-2, carries out electrostatic spinning, obtains nanofiber mats, then by fibrofelt thermal crosslinking treatment;
(3) above-mentioned nanofiber mats is infiltrated to 2-4h in water, then add the stable gold nano grain Au DSNPs aqueous solution of dendrimer, vibration, vacuum drying, obtains the PAA/PVA nanofiber mats containing Au DSNPs that physical method is assembled.
In described step (1), Polyamidoamine Dendrimers is the second generation.
In described step (1), preheating is in 60 DEG C of water-baths, preheating 20min.
In described step (1), the concentration of the Polyamidoamine Dendrimers aqueous solution is 2.5-3.5mM.
In described step (1), the concentration of chlorauric acid solution is 30mg/mL.
In described step (2), the total mass concentration of PAA/PVA is 12%.
In described step (2), electrostatic spinning process parameter is: spinning voltage 16.6kV, flow velocity 0.5mL/h, receiving range 25cm, humidity 40～60%, 20～25 DEG C of temperature.
In described step (2), heat cross-linking temperature is 120～145 DEG C, and crosslinking time is 30～45min.
The concentration of the stable gold nano grain Au DSNPs aqueous solution of dendrimer is 9～10.5mg/mL in described step (3).
In described step (1) and (3), be 24-36h drying time.
In described step (3), infiltrating time is 3h.
The catalytic performance of the complex fiber material of preparing for research step (3), by the PAA/PVA composite nano-fiber material containing Au DSNPs for the reduction reaction of catalysis tetranitro-phenol to verify its catalytic effect; Be assembled into gold nano grain catalytic activity on tunica fibrosa in order to contrast by physical method, must do one group of contrast, prepare the Au DSNPs aqueous solution with the same concentration of step (3), by chemical reaction, Au DSNPs is assembled on PAA/PVA tunica fibrosa, get supernatant Lambda25 ultraviolet-visible spectrophotometer after absorption and measure after these a series of absorption different times the Au DSNPs aqueous solution at the light absorption value at 520nm wavelength place, draw concentration-absorbance calibration curve, determine maximum chemical assembling absorption required time.The reduction reaction that fibrofelt after Chemical assembly is used for to catalysis tetranitro-phenol is to verify its catalytic effect.
The method of Chemical assembly fibrofelt is: 1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride (EDC) solution of preparation 5～6.3mg/mL, Static Spinning PAA/PVA fibrofelt is infiltrated to 3h in the EDC of 0.8～1.0mL solution, then add the Au DSNPs aqueous solution of 9～10.5mg/mL, shaking table vibration.After having assembled, take out tunica fibrosa vacuum drying, obtain the PAA/PVA fibrofelt containing Au DSNPs of chemical method assembling.
Use SEM(SEM), EDS(energy disperses spectrum), TEM(transmission electron microscope), TGA(thermogravimetric analysis), UV-vis(uv-vis spectra) characterize as follows respectively containing the stable composite nanometer fiber felt of gold nano grain of dendrimer and the result of catalytic activity thereof that the present invention obtains:
(1) test result of SEM
The test result of SEM shows: the PAA/PVA nanofiber mats that is assembled with Au DSNPs of preparing in the present invention pattern compared with the PAA/PVA nanofiber mats of unassembled Au DSNPs keeps good, and porosity is large, and fibre diameter is not found large change.Single nanofiber smooth surface, thickness is evenly distributed, without beading.The average fibre diameter of the PAA/PVA nanofiber mats of unassembled Au DSNPs is 225nm left and right, referring to accompanying drawing 1.The average fibre diameter that physical method is assembled with Au DSNPs is 225nm left and right, referring to accompanying drawing 2.The average fibre diameter that chemical method is assembled with Au DSNPs is 232nm left and right, referring to accompanying drawing 3.
(2) test result of EDS
The test result of EDS has confirmed to have gold element in Static Spinning PAA/PVA nanofiber mats that two kinds of assemble methods of physics and chemistry obtain, respectively referring to accompanying drawing 4(a), (b).
(3) TEM test result
TEM test result shows that in the fibrofelt obtaining by two kinds of assemble methods of physics and chemistry, gold nano grain is distributed in the surface of PAA/PVA nanofiber mats completely, and diameter is in 5nm left and right, referring to accompanying drawing 5.
(4) TGA test result
TGA test result shows: under air atmosphere, the PAA/PVA fibrofelt that contains Au DSNPs starts to be decomposed 200 DEG C of left and right.Experience after 900 DEG C of high temperature, two kinds of methods of physical absorption and chemical reaction are assembled the content that the final residue obtaining should be gold in fibrofelt.Show that by conversion the content of nanogold particle in fibrofelt is respectively 8.14% and 12%, referring to accompanying drawing 6.
(5) UV-vis test result
UV-vis test result shows: the surface plasma body resonant vibration absworption peak of nanogold particle has appearred in the fibrofelt that two kinds of methods of physical absorption and chemical reaction obtain at 536nm, referring to accompanying drawing 7.
The PAA/PVA nanofiber mats that contains Au DSNPs of assembling by physical method 8min left and right in the experiment of catalysis tetranitro-phenol reaches 97% catalytic efficiency, referring to accompanying drawing 8.Repeat 3 catalysis tetranitro-phenol description of tests by contrasting this material, this nanofiber mats still keeps the catalytic efficiency of stability and high efficiency, referring to accompanying drawing 9.And chemical method is assembled with 20min left and right under the PAA/PVA nanofiber mats same experimental conditions of Au DSNPs and reaches 98% catalytic efficiency, referring to accompanying drawing 10.Compare with the catalytic activity of the fibrofelt of physical method assembling, the catalytic activity of the fibrofelt of chemical method assembling slightly a little less than.Equally, chemical method is assembled with PAA/PVA nanofiber mats catalysis tetranitro-phenol experiment discovery in triplicate under same experimental conditions of Au DSNPs, and the stable catalytic efficiency of the same maintenance of this nanofiber mats, referring to accompanying drawing 11.
The present invention relates to 3 general principles:
(1) make full use of molecular structure and the surface characteristic of second generation Polyamidoamine Dendrimers, implement autoreduction and stabilization to nanogold particle, prevent the reunion of gold nano grain.
(2) physics assembling utilizes the negative electrical charge of polyacrylic carboxyl in nanofiber mats and the positive charge of dendrimer surface amino groups, thereby makes the stable gold nano grain Electrostatic Absorption of dendrimer to nanofiber mats surface.
(3) Chemical assembly is by with polyacrylic carboxyl in EDC activated fiber felt, then reacts with the amino on dendrimer surface and forms amido link, thereby gold nano grain stable dendrimer is assembled into fibrofelt surface.
beneficial effect
(1) preparation method of the present invention is simple, and easy operating adopts environmentally friendly macromolecular material, is applicable to suitability for industrialized production;
(2) the present invention is assembled into gold nano grain stable dendrimer on fibrofelt by two kinds of methods, there is not agglomeration in gold nano grain, obtain effectively fixingly, ensured that nanogold particle can recycle and can not be released in follow-up application;
(3) size of nanometer gold grain that prepared by the present invention is little, has splendid catalytic activity, has a extensive future.
Brief description of the drawings
Fig. 1 is the SEM figure of the Static Spinning PAA/PVA composite nanometer fiber felt prepared of the present invention;
Fig. 2 be the present invention prepare be assembled with the SEM figure of the Static Spinning PAA/PVA composite nanometer fiber felt of Au DSNPs by physical method;
Fig. 3 be the present invention prepare be assembled with the SEM figure of the Static Spinning PAA/PVA composite nanometer fiber felt of Au DSNPs by chemical method;
Fig. 4 is the EDS collection of illustrative plates that the physical method (a) prepared of the present invention and chemical method (b) are assembled with the Static Spinning PAA/PVA composite nanometer fiber felt of Au DSNPs;
Fig. 5 is cross section TEM picture and the gold nano grain particle diameter distribution histogram that the physical method (a) prepared of the present invention and chemical method (b) are assembled with the Static Spinning PAA/PVA composite nanometer fiber felt of Au DSNPs;
Fig. 6 is the TGA spectrogram of the Static Spinning PAA/PVA composite nanometer fiber felt that is loaded with Au DSNPs prepared of the present invention;
Fig. 7 is the solid uv atlas of the Static Spinning PAA/PVA composite nanometer fiber felt that is loaded with Au DSNPs prepared of the present invention;
Fig. 8 be the present invention prepare be assembled with the UV-vis spectrogram spectrum of the Static Spinning PAA/PVA composite nanometer fiber felt catalytic reduction tetranitro-phenol of Au DSNPs by physical method; A-m represents respectively the uv atlas at different time points (0,1,2,3,4,6,8,12,20,28,36min) tetranitro-phenol in catalysis tetranitro-phenol reduction experiment;
Fig. 9 be the present invention prepare by physical method be assembled with Au DSNPs Static Spinning PAA/PVA composite nanometer fiber felt catalytic reduction tetranitro-phenol repeat to test catalytic efficiency contrast figure for three times;
Figure 10 be the present invention prepare be assembled with the UV-vis spectrogram spectrum of the Static Spinning PAA/PVA composite nanometer fiber felt catalytic reduction tetranitro-phenol of Au DSNPs by chemical method; A-m represents respectively the uv atlas at different time points (0,1,2,3,4,6,8,12,20,28,36min) tetranitro-phenol in catalysis tetranitro-phenol reduction experiment;
Figure 11 be the present invention prepare by chemical method be assembled with Au DSNPs Static Spinning PAA/PVA composite nanometer fiber felt catalytic reduction tetranitro-phenol repeat to test catalytic efficiency contrast figure for three times.
Detailed description of the invention
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Get HAuCl 4100mg, is dissolved in distilled water, and magnetic force concussion makes it to be sufficiently uniformly dissolved, and is mixed with the solution that concentration is 30mg/mL.Get second generation Polyamidoamine Dendrimers (G2.NH 2) 162.97mg, being dissolved in 16mL distilled water, magnetic force concussion makes it to be sufficiently uniformly dissolved.This solution is placed in to 60 DEG C of water-bath preheating 20min.Get HAuCl 4solution 2.061mL, adds in preheated dendrimer solution.Temperature maintains 60 DEG C, magnetic agitation reaction 3.0h.After reaction finishes, gained solution is carried out to freeze drying processing, obtain the stable gold nano grain of dendrimer ,-20 DEG C of preservations.
The test result of TEM shows: the gold nano grain diameter of preparing taking Polyamidoamine Dendrimers as stabilisation carrier is evenly distributed, and average diameter is 5.5 ± 1.8nm.As accompanying drawing 5.
Embodiment 2
Take 12g polyvinyl alcohol in beaker, taking deionized water as solvent, 80 DEG C of constant temperature stir 3h.Be mixed with mass percent concentration and be 12% the PVA aqueous solution, cooling rear stand-by.Be mixed with the 10mL mixed solution of two kinds of polymer concentrations according to the ratio of PAA/PVA weight ratio 1:1.Spinning condition is set is: voltage 16.6kV, flow velocity 0.5mL/h, receiving range 25cm, humidity 40～60%, 20～25 DEG C of temperature.In spinning process, nanofiber deposits on aluminium foil and forms fibrofelt, by fibrofelt thermal crosslinking treatment 30min under the condition of 145 DEG C, obtains the fibrofelt that water stability is good.
Getting the stable gold nano grain of 4mg second generation polyamide-amine dendrimer is dissolved in and in 0.4mL deionized water, is mixed with the 10mg/mL aqueous solution.5mg PAA/PVA fibrofelt is immersed in to 3h in 0.8mL deionized water, then the stable gold nano grain aqueous solution of dendrimer that measures 0.2mL concentration and be 10mg/mL is added drop-wise on PAA/PVA fibrofelt, after absorption 20min, take out, washing, it after dry 24h, is placed in to vacuum drying chamber and preserves in vacuum drying chamber.The fibrofelt SEM that assembles gold nano grain by physical method obtaining characterizes, and average fibre diameter is 225nm left and right, referring to accompanying drawing 2.In the Static Spinning PAA/PVA nanofiber mats that the test result of EDS has confirmed to obtain, there is gold element, referring to accompanying drawing 4(a).In the fibrofelt that TEM test result shows to obtain, gold nano grain is distributed in the surface of PAA/PVA nanofiber mats completely, and diameter is in 5nm left and right, referring to accompanying drawing 5(a).TGA test result shows that the content of nanogold particle in fibrofelt is 8.14%, referring to accompanying drawing 6.UV-vis test result shows, the surface plasma body resonant vibration absworption peak of nanogold particle has appearred in fibrofelt at 536nm, referring to accompanying drawing 7.
Embodiment 3
Get 13.91mg tetranitro-phenol and be dissolved in magnetic agitation in 10mL methanol solution, be mixed with the light yellow tetranitro-phenol solution of 10mM; Get 37.87mg NaBH 4be mixed with the aqueous solution of 10M, stand-by; Preparation 0.6mL10mM tetranitro-phenol solution+0.6mL10M NaBH 4solution+16.8mL deionized water mixed solution, then the fibrofelt that physical method is assembled with to the stable gold nano grain of dendrimer is immersed in this mixed solution, keeping gold nano grain on fibrofelt is 0.025mg/mL with the ratio of the volume of mixed solution, fibrofelt carries out catalysis to tetranitro-phenol under magnetic agitation, respectively at 0min, 1min, 2min, 3min, 4min, 6min, 8min, 12min, 20min, 28min and 36min time point are respectively got the change in concentration of 0.5mL solution with test tetranitro-phenol.UV-vis test result shows, in the time of 8min, the absorption value that tetranitro-phenol is 400nm place characteristic peak at wavelength reduces rapidly, produces the characteristic peak of new catalysate para-aminophenol at 300nm place simultaneously, and corresponding catalytic efficiency also can reach 97%(as Fig. 8).The Static Spinning PAA/PVA composite nanometer fiber felt that contains Au DSNPs with same carries out repeating for three times experiment, by relatively finding its catalytic efficiency that can keep efficient stable (as Fig. 9).
Comparative example 1
Take 12g polyvinyl alcohol in beaker, taking deionized water as solvent, 80 DEG C of constant temperature stir 3h.Be mixed with mass percent concentration and be 12% the PVA aqueous solution, cooling rear stand-by.Be mixed with the 10mL mixed solution of two kinds of polymer concentrations according to the ratio of PAA/PVA weight ratio 1:1.Spinning condition is set is: voltage 16.6kV, flow velocity 0.5mL/h, receiving range 25cm, humidity 40～60%, 20～25 DEG C of temperature.In spinning process, nanofiber deposits to and on aluminium foil, forms fibrofelt; By fibrofelt thermal crosslinking treatment 30min under the condition of 145 DEG C, obtain the fibrofelt that water stability is good.
Getting the stable gold nano grain of 4mg second generation polyamide-amine dendrimer is dissolved in and in 0.4mL deionized water, is mixed with the 10mg/mL aqueous solution.Get 10mg1-(3-dimethylamino-propyl)-3-ethyl-carbodiimide hydrochloride (EDC) and be dissolved in 1.6mL deionized water, be made into the EDC solution of 6.25mg/mL.The EDC solution 0.8mL that measures 6.25mg/mL infiltrates 5mg PAA/PVA tunica fibrosa, the carboxyl 3h of activated polyacrylic acid, and then adding 0.2mL concentration is the stable gold nano grain aqueous solution of 10mg/mL second generation polyamide-amine dendrimer.After reaction 2d, take out on PAA/PVA fibrofelt, washing, is placed in vacuum drying chamber dry after 24 hours, is placed in vacuum drying chamber and preserves.The fibrofelt SEM that assembles gold nano grain by chemical method obtaining characterizes, and average fibre diameter is 232nm left and right, referring to accompanying drawing 3.In the Static Spinning PAA/PVA nanofiber mats that the test result of EDS has confirmed to obtain, there is gold element, referring to accompanying drawing 4(b).In the fibrofelt that TEM test result shows to obtain, gold nano grain is distributed in the surface of PAA/PVA nanofiber mats completely, and diameter is in 5nm left and right, referring to accompanying drawing 5(b).TGA test result shows that the content of nanogold particle in fibrofelt is 8.14%, referring to accompanying drawing 6.UV-vis test result shows, the surface plasma body resonant vibration absworption peak of nanogold particle has appearred in fibrofelt at 536nm, referring to accompanying drawing 7.
Comparative example 2
Get 13.91mg tetranitro-phenol and be dissolved in magnetic agitation in 10mL methanol solution, be mixed with the light yellow tetranitro-phenol solution of 10mM; Get 37.87mgNaBH 4be mixed with the aqueous solution of 10M, stand-by.Preparation 0.6mL10mM tetranitro-phenol+0.6ML10M NaBH 4+ 16.8mL deionized water mixed solution, is then immersed in the fibrofelt that is assembled with the stable gold nano grain of dendrimer by chemical method in this mixed solution, and keeping gold nano grain on fibrofelt is 0.025mg/mL with the ratio of the volume of mixed solution.Fibrofelt carries out catalysis to tetranitro-phenol under magnetic agitation, respectively at 0min, and 1min, 2min, 3min, 4min, 6min, 8min, 12min, 20min, 28min and 36min time point are respectively got the variable quantity of 0.5ml solution with test tetranitro-phenol.UV-vis test result shows, in the time of 8min, the catalytic efficiency of tetranitro-phenol is only 64%.In the time of 20min, the absorption value that tetranitro-phenol is 400nm place characteristic peak at wavelength reduces rapidly, produces the characteristic peak of new catalysate p-aminophenol at 300nm place simultaneously, and corresponding catalytic efficiency just reaches 97%(as Figure 10).The Static Spinning PAA/PVA composite nanometer fiber felt that contains Au DSNPs with same carries out repeating for three times experiment, by relatively finding that it can keep stable catalytic efficiency (as Figure 11).

Claims (9)

1. a preparation method who contains the PAA/PVA nanofiber mats of Au DSNPs, comprising:
(1) by the preheating of the Polyamidoamine Dendrimers aqueous solution, then add chlorauric acid solution, stirring reaction 2-3h, cool drying, obtains the stable gold nano grain Au DSNPs of dendrimer; Wherein the mol ratio of gold and dendrimer is 3:1; Wherein Polyamidoamine Dendrimers is the second generation; Preheating is in 60 DEG C of water-baths, preheating 20min;
(2) the polyelectrolyte spinning solution of the polyacrylic acid PAA/ PVAC polyvinylalcohol that preparation weight ratio is 1:1-2, carries out electrostatic spinning, obtains nanofiber mats, then by fibrofelt thermal crosslinking treatment;
(3) above-mentioned nanofiber mats is infiltrated to 2-4h in water, then add the stable gold nano grain Au DSNPs aqueous solution of dendrimer, vibration, vacuum drying, obtains the PAA/PVA nanofiber mats containing Au DSNPs.
2. the preparation method of a kind of PAA/PVA nanofiber mats containing Au DSNPs according to claim 1, is characterized in that: in described step (1), the concentration of the Polyamidoamine Dendrimers aqueous solution is 2.5-3.5mM.
3. the preparation method of a kind of PAA/PVA nanofiber mats containing Au DSNPs according to claim 1, is characterized in that: in described step (1), the concentration of chlorauric acid solution is 30mg/mL.
4. the preparation method of a kind of PAA/PVA nanofiber mats containing Au DSNPs according to claim 1, is characterized in that: in described step (2), the total mass concentration of PAA/PVA is 12%.
5. the preparation method of a kind of PAA/PVA nanofiber mats containing Au DSNPs according to claim 1, it is characterized in that: in described step (2), electrostatic spinning process parameter is: spinning voltage 16.6kV, flow velocity 0.5mL/h, receiving range 25cm, humidity 40～60%, 20～25 DEG C of temperature.
6. the preparation method of a kind of PAA/PVA nanofiber mats containing Au DSNPs according to claim 1, is characterized in that: in described step (2), heat cross-linking temperature is 120～145 DEG C, and crosslinking time is 30～45min.
7. the preparation method of a kind of PAA/PVA nanofiber mats containing Au DSNPs according to claim 1, is characterized in that: in described step (3), the concentration of the stable gold nano grain Au DSNPs aqueous solution of dendrimer is 9～10.5mg/mL.
8. the preparation method of a kind of PAA/PVA nanofiber mats containing Au DSNPs according to claim 1, is characterized in that: in described step (1) and (3), be 24-36h drying time.
9. the preparation method of a kind of PAA/PVA nanofiber mats containing Au DSNPs according to claim 1, is characterized in that: in described step (3), infiltrating time is 3h.
CN201310067293.0A 2013-03-04 2013-03-04 Method for preparing phenolic aldehyde amine (PAA)/polyvinyl acetate (PVA) nano-fiber felt containing Au dendrimer-stabilized nanoparticles (DSNPs) Expired - Fee Related CN103143392B (en)

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